反应详情

4-chloro-4'-mercaptomethylbenzophenone (14.7 g) and potassium hydroxide (15 g) was added to a solvent comprising dioxane (100 ml) and water (100 ml). Difluoromethyl chloride was blown into this solution at 60° C. until the starting material 4-chloro-4'-mercaptomethylbenzophenone disappeared. The reaction product was cooled to room temperature and then subjected to filtration. The organic layer as the filtrate was dried over anhydrous magnesium sulfate add concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to obtain the desired product (6.4 g, melting point: 34° to 35° C., yield: 36%).

1. filtrationsubjected to filtration
2. dry with materialThe organic layer as the filtrate was dried over anhydrous magnesium sulfate
3. additionadd
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)